Abstract: Objectives A method for the simult aneous determination of methyl chlorides(dichloromethane,trichlor omethane and tetrachloro methane)and BTEX(benzene,toluene,ethylbenzene and xylenes isomers)in env ironmental samples were studied using headspace solid-phase micro-extraction(SPME)and gas chromatography.Methods Solid phase microextraction with uncoated fiber in the headspace and capillary gas chromatography were used to determinate methyl chlorides and BTEX.The extractive and chromatog raphic conditions were optimized.Results Linear limits of the method: dichlormethane 0.14-75.7μg/L,trichloromethane 0 24-84.5μg/L,tetrachlor methane 0.45-137.1μg/L,benzene 0.03 -12.6μg/L,toluene 0.10-24.8μg/L,ethylbenzene 0.06-24.7μg/L,xylenes isomers 0.13-24.8μg/L.The cofficient of correlation ranged form 0.991 5-0.997 9,limit of detection of volatiles above were 0.14μg/L、0.24μg/L、0.45μg/L、0.03μg/L、0.10μg/L、0.06μg/L、0.13μg/L.The recoveries and coefficient of variation in sample determination ranged from 80.0%-111.6% and from 4.4%-8.1%,respectively.Conclusion This method was simple,fast,accurate with high reproducibility,high sensitivity and low cost.